An iron(II) complex tripodally chelated with 1,1,1-tris­(pyridin-2-yl)ethane showing room-temperature spin-crossover behaviour

The spin-crossover phenomenon is a reversible low- and high-spin transition caused by external stimuli such as heat. In the novel iron(II) complex salt tetra­phenyl­phospho­nium tris­(thio­cyanato-[kappa]N)[1,1,1-tris­(pyridin-2-yl)ethane-[kappa]³N,N',N'']ferrate(II), (C₂₄H₂₀P)[Fe(NCS)₃(C₁₇H₁₅N₃)], the Fe-N bond lengths are in the range 2.027 (2)-2.089 (2) Å, indicating that the specimen consists of comparable molar fractions of the low- and high-spin species at 296 K. A magnetic study confirmed that spin-crossover takes place at around 290 K.

Computing details

Data collection: CrystalClear (Rigaku/MSC, 2006) for I100K; RAPID-AUTO (Rigaku, 1998) for I296K. Cell refinement: CrystalClear (Rigaku/MSC, 2006) for I100K; RAPID-AUTO (Rigaku, 1998) for I296K. Data reduction: CrystalClear (Rigaku/MSC, 2006) for I100K; RAPID-AUTO (Rigaku, 1998) for I296K. For both compounds, program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: CrystalStructure (Rigaku, 2015). Software used to prepare material for publication: CrystalStructure (Rigaku, 2015) and CRYSTALS (Carruthers et al., 1999) for I100K; CrystalStructure (Rigaku, 2015) for I296K.

(I100K) Tetraphenylphosphonium tris(thiocyanato-κN)[1,1,1-tris(pyridin-2-yl)ethane-κ³N,N',N'']ferrate(II)

Crystal data

(C24H20P)[Fe(NCS)3(C17H15N3)]	F(000) = 1720.00
Mr = 830.78	Dx = 1.376 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 8.9560 (11) Å	Cell parameters from 17570 reflections
b = 15.7745 (16) Å	θ = 1.3–27.5°
c = 28.455 (3) Å	µ = 0.61 mm^−1
β = 94.067 (3)°	T = 100 K
V = 4009.9 (8) Å^3	Platelet, red
Z = 4	0.27 × 0.25 × 0.19 mm

Data collection

Rigaku Saturn70 diffractometer	7802 reflections with F^2 > 2.0σ(F^2)
Detector resolution: 14.629 pixels mm^-1	Rint = 0.100
ω scans	θmax = 27.5°, θmin = 1.4°
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	h = −11→11
Tmin = 0.750, Tmax = 0.890	k = −20→20
64292 measured reflections	l = −36→36
9165 independent reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.057	H-atom parameters constrained
wR(F^2) = 0.158	w = 1/[σ^2(Fo^2) + (0.08P)^2 + 1.4P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.002
9165 reflections	Δρmax = 0.50 e Å^−3
497 parameters	Δρmin = −0.66 e Å^−3
0 restraints	Extinction correction: SHELXL2014 (Sheldrick, 2015)
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0027 (6)
Secondary atom site location: difference Fourier map

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	1.00601 (4)	0.23930 (2)	0.39872 (2)	0.01919 (13)
S1	1.37039 (8)	0.34151 (4)	0.51485 (2)	0.02815 (18)
S2	1.33564 (7)	0.00744 (4)	0.37939 (2)	0.02718 (18)
S3	1.24779 (9)	0.41893 (5)	0.29437 (3)	0.0349 (2)
P1	0.96659 (8)	0.24231 (4)	0.15041 (2)	0.01964 (16)
N1	0.8755 (2)	0.33758 (13)	0.40150 (7)	0.0199 (4)
N2	0.8686 (2)	0.19120 (13)	0.34949 (7)	0.0184 (4)
N3	0.8866 (2)	0.18275 (13)	0.44458 (7)	0.0198 (4)
N4	1.1417 (2)	0.28445 (14)	0.44967 (8)	0.0249 (5)
N5	1.1361 (2)	0.14012 (14)	0.39498 (8)	0.0246 (5)
N6	1.1168 (2)	0.29979 (14)	0.35215 (8)	0.0238 (5)
C1	0.6661 (3)	0.23700 (16)	0.39786 (9)	0.0200 (5)
C2	0.7253 (3)	0.32819 (16)	0.39921 (9)	0.0213 (5)
C3	0.6316 (3)	0.39854 (18)	0.39991 (10)	0.0292 (6)
H3	0.5261	0.3912	0.3971	0.035*
C4	0.6917 (3)	0.47899 (18)	0.40468 (10)	0.0306 (6)
H4	0.6284	0.5272	0.4053	0.037*
C5	0.8457 (3)	0.48803 (17)	0.40846 (9)	0.0279 (6)
H5	0.8899	0.5425	0.4127	0.034*
C6	0.9338 (3)	0.41702 (16)	0.40601 (9)	0.0247 (6)
H6	1.0394	0.4237	0.4075	0.030*
C7	0.7198 (3)	0.19003 (15)	0.35489 (8)	0.0188 (5)
C8	0.6223 (3)	0.14367 (17)	0.32427 (9)	0.0240 (5)
H8	0.5182	0.1423	0.3288	0.029*
C9	0.6785 (3)	0.09954 (18)	0.28719 (9)	0.0265 (6)
H9	0.6135	0.0669	0.2665	0.032*
C10	0.8290 (3)	0.10329 (17)	0.28063 (9)	0.0257 (6)
H10	0.8693	0.0744	0.2551	0.031*
C11	0.9202 (3)	0.15013 (16)	0.31204 (9)	0.0231 (5)
H11	1.0238	0.1537	0.3072	0.028*
C12	0.7355 (3)	0.18971 (15)	0.44137 (9)	0.0204 (5)
C13	0.6498 (3)	0.15393 (18)	0.47505 (10)	0.0289 (6)
H13	0.5444	0.1618	0.4731	0.035*
C14	0.7188 (3)	0.10683 (18)	0.51140 (10)	0.0327 (7)
H14	0.6613	0.0814	0.5344	0.039*
C15	0.8727 (4)	0.09736 (18)	0.51380 (10)	0.0314 (6)
H15	0.9224	0.0644	0.5381	0.038*
C16	0.9527 (3)	0.13669 (16)	0.48031 (9)	0.0256 (6)
H16	1.0586	0.1312	0.4825	0.031*
C17	0.4954 (3)	0.23621 (18)	0.39694 (9)	0.0254 (6)
H17A	0.4597	0.1775	0.3961	0.030*
H17B	0.4634	0.2643	0.4253	0.030*
H17C	0.4537	0.2664	0.3689	0.030*
C18	1.2354 (3)	0.30851 (17)	0.47725 (9)	0.0218 (5)
C19	1.2182 (3)	0.08400 (16)	0.38895 (9)	0.0216 (5)
C20	1.1717 (3)	0.34882 (17)	0.32823 (9)	0.0236 (5)
C21	0.8236 (3)	0.28566 (16)	0.18457 (9)	0.0236 (5)
C22	0.6798 (3)	0.29939 (18)	0.16348 (10)	0.0292 (6)
H22	0.6583	0.2876	0.1310	0.035*
C23	0.5693 (3)	0.33015 (19)	0.19024 (12)	0.0364 (7)
H23	0.4717	0.3399	0.1760	0.044*
C24	0.5995 (4)	0.34703 (18)	0.23778 (12)	0.0371 (7)
H24	0.5223	0.3675	0.2560	0.045*
C25	0.7413 (3)	0.33418 (17)	0.25852 (11)	0.0329 (7)
H25	0.7618	0.3462	0.2911	0.039*
C26	0.8539 (3)	0.30394 (16)	0.23226 (9)	0.0263 (6)
H26	0.9518	0.2956	0.2467	0.032*
C27	0.8778 (3)	0.17517 (16)	0.10591 (9)	0.0224 (5)
C28	0.7801 (3)	0.11190 (18)	0.11959 (10)	0.0279 (6)
H28	0.7559	0.1081	0.1515	0.033*
C29	0.7186 (3)	0.05482 (19)	0.08660 (11)	0.0340 (7)
H29	0.6544	0.0110	0.0961	0.041*
C30	0.7511 (3)	0.06173 (19)	0.03946 (11)	0.0367 (7)
H30	0.7086	0.0230	0.0167	0.044*
C31	0.8455 (3)	0.12544 (19)	0.02613 (10)	0.0342 (7)
H31	0.8670	0.1303	−0.0060	0.041*
C32	0.9090 (3)	0.18221 (17)	0.05874 (9)	0.0277 (6)
H32	0.9735	0.2257	0.0491	0.033*
C33	1.0764 (3)	0.32355 (16)	0.12558 (9)	0.0214 (5)
C34	1.0457 (3)	0.40943 (16)	0.13257 (9)	0.0236 (5)
H34	0.9630	0.4259	0.1496	0.028*
C35	1.1380 (3)	0.47044 (17)	0.11423 (9)	0.0269 (6)
H35	1.1183	0.5289	0.1188	0.032*
C36	1.2579 (3)	0.44605 (18)	0.08946 (10)	0.0298 (6)
H36	1.3208	0.4881	0.0774	0.036*
C37	1.2877 (3)	0.36094 (18)	0.08195 (10)	0.0301 (6)
H37	1.3690	0.3450	0.0641	0.036*
C38	1.1986 (3)	0.29934 (17)	0.10049 (10)	0.0272 (6)
H38	1.2202	0.2410	0.0962	0.033*
C39	1.0934 (3)	0.18138 (16)	0.18876 (9)	0.0218 (5)
C40	1.0797 (3)	0.09412 (17)	0.19354 (9)	0.0246 (6)
H40	1.0079	0.0638	0.1739	0.030*
C41	1.1713 (3)	0.05133 (18)	0.22700 (10)	0.0293 (6)
H41	1.1615	−0.0083	0.2304	0.035*
C42	1.2763 (3)	0.09480 (19)	0.25535 (10)	0.0305 (6)
H42	1.3378	0.0652	0.2784	0.037*
C43	1.2925 (3)	0.18174 (19)	0.25030 (10)	0.0314 (6)
H43	1.3659	0.2113	0.2697	0.038*
C44	1.2020 (3)	0.22562 (18)	0.21698 (9)	0.0268 (6)
H44	1.2135	0.2851	0.2133	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0172 (2)	0.0191 (2)	0.0212 (2)	−0.00085 (14)	0.00131 (15)	−0.00053 (13)
S1	0.0277 (4)	0.0297 (4)	0.0262 (4)	−0.0044 (3)	−0.0035 (3)	−0.0037 (3)
S2	0.0271 (4)	0.0231 (3)	0.0321 (4)	0.0049 (3)	0.0078 (3)	0.0044 (3)
S3	0.0429 (5)	0.0246 (4)	0.0397 (4)	−0.0008 (3)	0.0193 (3)	0.0037 (3)
P1	0.0208 (3)	0.0187 (3)	0.0194 (3)	0.0001 (3)	0.0014 (2)	0.0014 (2)
N1	0.0202 (10)	0.0217 (11)	0.0177 (10)	−0.0020 (9)	0.0007 (8)	−0.0008 (8)
N2	0.0175 (10)	0.0171 (10)	0.0208 (10)	0.0015 (8)	0.0031 (8)	0.0018 (8)
N3	0.0223 (11)	0.0175 (10)	0.0193 (10)	0.0013 (9)	−0.0014 (8)	−0.0016 (8)
N4	0.0212 (11)	0.0260 (12)	0.0276 (12)	0.0017 (10)	0.0032 (9)	−0.0006 (9)
N5	0.0214 (11)	0.0268 (12)	0.0255 (11)	−0.0027 (10)	0.0006 (9)	−0.0018 (9)
N6	0.0194 (11)	0.0230 (11)	0.0293 (12)	0.0008 (9)	0.0032 (9)	−0.0039 (9)
C1	0.0195 (13)	0.0190 (12)	0.0218 (12)	−0.0016 (10)	0.0041 (10)	−0.0016 (10)
C2	0.0211 (12)	0.0219 (13)	0.0207 (12)	0.0000 (10)	0.0005 (10)	−0.0014 (10)
C3	0.0249 (14)	0.0280 (14)	0.0346 (15)	0.0016 (12)	0.0015 (11)	−0.0039 (12)
C4	0.0337 (16)	0.0210 (13)	0.0368 (16)	0.0046 (12)	0.0010 (12)	−0.0025 (12)
C5	0.0369 (16)	0.0187 (13)	0.0286 (14)	−0.0029 (12)	0.0050 (11)	−0.0019 (11)
C6	0.0304 (14)	0.0208 (13)	0.0230 (13)	−0.0067 (11)	0.0043 (10)	0.0012 (10)
C7	0.0203 (12)	0.0159 (11)	0.0204 (12)	0.0004 (10)	0.0025 (9)	0.0020 (9)
C8	0.0221 (13)	0.0249 (13)	0.0247 (13)	−0.0011 (11)	−0.0006 (10)	−0.0013 (10)
C9	0.0281 (14)	0.0282 (14)	0.0229 (13)	−0.0041 (12)	−0.0012 (10)	−0.0030 (11)
C10	0.0308 (14)	0.0245 (13)	0.0226 (13)	−0.0013 (11)	0.0071 (11)	−0.0026 (10)
C11	0.0214 (13)	0.0240 (13)	0.0243 (13)	−0.0001 (11)	0.0049 (10)	0.0019 (10)
C12	0.0233 (13)	0.0170 (12)	0.0212 (12)	−0.0006 (10)	0.0027 (9)	−0.0016 (10)
C13	0.0317 (15)	0.0300 (15)	0.0258 (14)	−0.0035 (12)	0.0083 (11)	−0.0015 (11)
C14	0.0459 (18)	0.0282 (15)	0.0250 (14)	−0.0071 (13)	0.0091 (12)	0.0030 (11)
C15	0.0459 (18)	0.0253 (14)	0.0226 (13)	0.0002 (13)	−0.0012 (12)	−0.0004 (11)
C16	0.0317 (15)	0.0214 (13)	0.0232 (13)	0.0025 (11)	−0.0030 (10)	−0.0024 (10)
C17	0.0187 (13)	0.0286 (14)	0.0294 (15)	−0.0021 (11)	0.0054 (11)	−0.0072 (11)
C18	0.0205 (13)	0.0231 (13)	0.0220 (12)	−0.0001 (10)	0.0030 (10)	0.0010 (10)
C19	0.0193 (12)	0.0210 (13)	0.0247 (13)	−0.0035 (11)	0.0016 (10)	0.0022 (10)
C20	0.0203 (12)	0.0238 (13)	0.0269 (13)	0.0019 (11)	0.0031 (10)	−0.0024 (11)
C21	0.0258 (14)	0.0181 (12)	0.0278 (13)	−0.0008 (11)	0.0073 (10)	0.0039 (10)
C22	0.0246 (14)	0.0293 (15)	0.0338 (15)	−0.0007 (12)	0.0031 (11)	0.0018 (12)
C23	0.0267 (15)	0.0320 (16)	0.0514 (19)	0.0021 (13)	0.0095 (13)	0.0036 (14)
C24	0.0370 (17)	0.0254 (15)	0.0520 (19)	0.0020 (13)	0.0243 (14)	0.0021 (13)
C25	0.0464 (18)	0.0205 (13)	0.0336 (15)	−0.0004 (13)	0.0162 (13)	0.0007 (11)
C26	0.0325 (15)	0.0198 (13)	0.0272 (14)	−0.0015 (11)	0.0060 (11)	−0.0007 (10)
C27	0.0224 (13)	0.0191 (12)	0.0251 (13)	0.0020 (10)	−0.0024 (10)	0.0002 (10)
C28	0.0241 (14)	0.0293 (14)	0.0302 (14)	−0.0018 (12)	0.0011 (11)	0.0004 (11)
C29	0.0280 (15)	0.0280 (15)	0.0450 (18)	−0.0028 (12)	−0.0041 (12)	−0.0010 (13)
C30	0.0408 (17)	0.0304 (15)	0.0365 (16)	0.0016 (14)	−0.0150 (13)	−0.0079 (13)
C31	0.0442 (18)	0.0308 (15)	0.0262 (14)	0.0030 (14)	−0.0072 (12)	−0.0026 (12)
C32	0.0386 (16)	0.0194 (13)	0.0246 (13)	0.0013 (12)	−0.0016 (11)	0.0024 (10)
C33	0.0226 (13)	0.0196 (12)	0.0217 (12)	0.0003 (10)	0.0001 (10)	0.0016 (10)
C34	0.0266 (14)	0.0248 (13)	0.0192 (12)	0.0017 (11)	0.0006 (10)	−0.0006 (10)
C35	0.0302 (14)	0.0210 (13)	0.0291 (14)	−0.0039 (11)	−0.0011 (11)	0.0002 (11)
C36	0.0289 (14)	0.0285 (14)	0.0318 (15)	−0.0090 (12)	0.0014 (11)	0.0050 (12)
C37	0.0291 (15)	0.0302 (15)	0.0317 (15)	0.0006 (12)	0.0076 (11)	0.0039 (12)
C38	0.0291 (15)	0.0214 (13)	0.0320 (14)	0.0035 (11)	0.0075 (11)	0.0016 (11)
C39	0.0223 (13)	0.0225 (13)	0.0208 (12)	0.0013 (11)	0.0043 (10)	0.0026 (10)
C40	0.0281 (14)	0.0223 (13)	0.0236 (13)	0.0019 (11)	0.0038 (10)	−0.0007 (10)
C41	0.0318 (15)	0.0235 (14)	0.0326 (15)	0.0036 (12)	0.0026 (12)	0.0038 (11)
C42	0.0241 (14)	0.0383 (16)	0.0289 (14)	0.0049 (12)	0.0008 (11)	0.0085 (12)
C43	0.0264 (14)	0.0361 (16)	0.0313 (15)	−0.0034 (13)	−0.0013 (11)	0.0017 (12)
C44	0.0267 (14)	0.0261 (14)	0.0273 (14)	−0.0021 (12)	0.0003 (11)	0.0030 (11)

Geometric parameters (Å, º)

Fe1—N1	1.946 (2)	C16—H16	0.9500
Fe1—N2	1.952 (2)	C17—H17A	0.9800
Fe1—N3	1.959 (2)	C17—H17B	0.9800
Fe1—N4	1.959 (2)	C17—H17C	0.9800
Fe1—N5	1.958 (2)	C21—C26	1.395 (4)
Fe1—N6	1.959 (2)	C21—C22	1.399 (4)
S1—C18	1.642 (3)	C22—C23	1.379 (4)
S2—C19	1.637 (3)	C22—H22	0.9500
S3—C20	1.646 (3)	C23—C24	1.386 (5)
P1—C33	1.791 (3)	C23—H23	0.9500
P1—C27	1.793 (3)	C24—C25	1.377 (5)
P1—C39	1.797 (3)	C24—H24	0.9500
P1—C21	1.797 (3)	C25—C26	1.382 (4)
N1—C2	1.351 (3)	C25—H25	0.9500
N1—C6	1.360 (3)	C26—H26	0.9500
N2—C7	1.352 (3)	C27—C32	1.395 (4)
N2—C11	1.356 (3)	C27—C28	1.401 (4)
N3—C16	1.351 (3)	C28—C29	1.386 (4)
N3—C12	1.355 (3)	C28—H28	0.9500
N4—C18	1.170 (3)	C29—C30	1.397 (4)
N5—C19	1.171 (3)	C29—H29	0.9500
N6—C20	1.162 (3)	C30—C31	1.384 (4)
C1—C17	1.527 (4)	C30—H30	0.9500
C1—C2	1.532 (3)	C31—C32	1.383 (4)
C1—C7	1.536 (3)	C31—H31	0.9500
C1—C12	1.538 (3)	C32—H32	0.9500
C2—C3	1.392 (4)	C33—C34	1.399 (4)
C3—C4	1.381 (4)	C33—C38	1.401 (4)
C3—H3	0.9500	C34—C35	1.394 (4)
C4—C5	1.383 (4)	C34—H34	0.9500
C4—H4	0.9500	C35—C36	1.380 (4)
C5—C6	1.375 (4)	C35—H35	0.9500
C5—H5	0.9500	C36—C37	1.388 (4)
C6—H6	0.9500	C36—H36	0.9500
C7—C8	1.396 (3)	C37—C38	1.385 (4)
C8—C9	1.388 (4)	C37—H37	0.9500
C8—H8	0.9500	C38—H38	0.9500
C9—C10	1.375 (4)	C39—C40	1.390 (4)
C9—H9	0.9500	C39—C44	1.403 (4)
C10—C11	1.381 (4)	C40—C41	1.387 (4)
C10—H10	0.9500	C40—H40	0.9500
C11—H11	0.9500	C41—C42	1.378 (4)
C12—C13	1.389 (4)	C41—H41	0.9500
C13—C14	1.383 (4)	C42—C43	1.388 (4)
C13—H13	0.9500	C42—H42	0.9500
C14—C15	1.383 (4)	C43—C44	1.388 (4)
C14—H14	0.9500	C43—H43	0.9500
C15—C16	1.380 (4)	C44—H44	0.9500
C15—H15	0.9500
N1—Fe1—N2	89.36 (8)	C15—C16—H16	118.6
N1—Fe1—N5	179.15 (9)	C1—C17—H17A	109.5
N2—Fe1—N5	89.86 (9)	C1—C17—H17B	109.5
N1—Fe1—N4	91.33 (9)	H17A—C17—H17B	109.5
N2—Fe1—N4	177.96 (9)	C1—C17—H17C	109.5
N5—Fe1—N4	89.46 (9)	H17A—C17—H17C	109.5
N1—Fe1—N6	88.50 (9)	H17B—C17—H17C	109.5
N2—Fe1—N6	91.59 (9)	N4—C18—S1	178.3 (2)
N5—Fe1—N6	91.18 (9)	N5—C19—S2	178.2 (2)
N4—Fe1—N6	90.35 (9)	N6—C20—S3	179.4 (3)
N1—Fe1—N3	88.74 (9)	C26—C21—C22	119.7 (2)
N2—Fe1—N3	87.41 (8)	C26—C21—P1	120.5 (2)
N5—Fe1—N3	91.56 (9)	C22—C21—P1	119.8 (2)
N4—Fe1—N3	90.68 (9)	C23—C22—C21	119.5 (3)
N6—Fe1—N3	177.08 (9)	C23—C22—H22	120.2
C33—P1—C27	111.88 (12)	C21—C22—H22	120.2
C33—P1—C39	106.32 (12)	C22—C23—C24	120.6 (3)
C27—P1—C39	110.03 (12)	C22—C23—H23	119.7
C33—P1—C21	111.93 (12)	C24—C23—H23	119.7
C27—P1—C21	108.02 (12)	C25—C24—C23	120.0 (3)
C39—P1—C21	108.61 (12)	C25—C24—H24	120.0
C2—N1—C6	118.7 (2)	C23—C24—H24	120.0
C2—N1—Fe1	120.64 (17)	C24—C25—C26	120.4 (3)
C6—N1—Fe1	120.68 (17)	C24—C25—H25	119.8
C7—N2—C11	118.4 (2)	C26—C25—H25	119.8
C7—N2—Fe1	120.01 (16)	C25—C26—C21	119.9 (3)
C11—N2—Fe1	121.14 (17)	C25—C26—H26	120.1
C16—N3—C12	118.4 (2)	C21—C26—H26	120.1
C16—N3—Fe1	121.03 (18)	C32—C27—C28	119.7 (2)
C12—N3—Fe1	120.53 (16)	C32—C27—P1	121.6 (2)
C18—N4—Fe1	172.6 (2)	C28—C27—P1	118.6 (2)
C19—N5—Fe1	173.8 (2)	C29—C28—C27	120.1 (3)
C20—N6—Fe1	167.4 (2)	C29—C28—H28	120.0
C17—C1—C2	110.6 (2)	C27—C28—H28	120.0
C17—C1—C7	110.6 (2)	C28—C29—C30	120.0 (3)
C2—C1—C7	110.2 (2)	C28—C29—H29	120.0
C17—C1—C12	110.9 (2)	C30—C29—H29	120.0
C2—C1—C12	108.4 (2)	C31—C30—C29	119.5 (3)
C7—C1—C12	106.0 (2)	C31—C30—H30	120.2
N1—C2—C3	120.7 (2)	C29—C30—H30	120.2
N1—C2—C1	116.5 (2)	C30—C31—C32	121.1 (3)
C3—C2—C1	122.8 (2)	C30—C31—H31	119.4
C4—C3—C2	120.2 (3)	C32—C31—H31	119.4
C4—C3—H3	119.9	C31—C32—C27	119.5 (3)
C2—C3—H3	119.9	C31—C32—H32	120.2
C3—C4—C5	118.8 (3)	C27—C32—H32	120.2
C3—C4—H4	120.6	C34—C33—C38	120.3 (2)
C5—C4—H4	120.6	C34—C33—P1	121.18 (19)
C6—C5—C4	119.0 (3)	C38—C33—P1	118.5 (2)
C6—C5—H5	120.5	C35—C34—C33	119.2 (2)
C4—C5—H5	120.5	C35—C34—H34	120.4
N1—C6—C5	122.5 (2)	C33—C34—H34	120.4
N1—C6—H6	118.7	C36—C35—C34	120.1 (3)
C5—C6—H6	118.7	C36—C35—H35	119.9
N2—C7—C8	120.9 (2)	C34—C35—H35	119.9
N2—C7—C1	116.8 (2)	C35—C36—C37	120.9 (3)
C8—C7—C1	122.2 (2)	C35—C36—H36	119.6
C9—C8—C7	119.5 (2)	C37—C36—H36	119.6
C9—C8—H8	120.2	C38—C37—C36	119.8 (3)
C7—C8—H8	120.2	C38—C37—H37	120.1
C10—C9—C8	119.6 (2)	C36—C37—H37	120.1
C10—C9—H9	120.2	C37—C38—C33	119.6 (3)
C8—C9—H9	120.2	C37—C38—H38	120.2
C9—C10—C11	118.4 (2)	C33—C38—H38	120.2
C9—C10—H10	120.8	C40—C39—C44	120.0 (2)
C11—C10—H10	120.8	C40—C39—P1	122.2 (2)
N2—C11—C10	123.0 (2)	C44—C39—P1	117.7 (2)
N2—C11—H11	118.5	C41—C40—C39	119.8 (3)
C10—C11—H11	118.5	C41—C40—H40	120.1
N3—C12—C13	121.3 (2)	C39—C40—H40	120.1
N3—C12—C1	116.0 (2)	C42—C41—C40	120.4 (3)
C13—C12—C1	122.7 (2)	C42—C41—H41	119.8
C14—C13—C12	119.6 (3)	C40—C41—H41	119.8
C14—C13—H13	120.2	C41—C42—C43	120.2 (3)
C12—C13—H13	120.2	C41—C42—H42	119.9
C13—C14—C15	119.1 (3)	C43—C42—H42	119.9
C13—C14—H14	120.5	C44—C43—C42	120.2 (3)
C15—C14—H14	120.5	C44—C43—H43	119.9
C16—C15—C14	118.8 (3)	C42—C43—H43	119.9
C16—C15—H15	120.6	C43—C44—C39	119.4 (3)
C14—C15—H15	120.6	C43—C44—H44	120.3
N3—C16—C15	122.7 (3)	C39—C44—H44	120.3
N3—C16—H16	118.6
C6—N1—C2—C3	2.1 (4)	C33—P1—C21—C22	93.5 (2)
Fe1—N1—C2—C3	−178.26 (19)	C27—P1—C21—C22	−30.1 (2)
C6—N1—C2—C1	−175.6 (2)	C39—P1—C21—C22	−149.4 (2)
Fe1—N1—C2—C1	4.1 (3)	C26—C21—C22—C23	−0.6 (4)
C17—C1—C2—N1	178.1 (2)	P1—C21—C22—C23	178.0 (2)
C7—C1—C2—N1	−59.2 (3)	C21—C22—C23—C24	−0.4 (4)
C12—C1—C2—N1	56.4 (3)	C22—C23—C24—C25	0.9 (5)
C17—C1—C2—C3	0.6 (3)	C23—C24—C25—C26	−0.4 (4)
C7—C1—C2—C3	123.2 (3)	C24—C25—C26—C21	−0.5 (4)
C12—C1—C2—C3	−121.2 (3)	C22—C21—C26—C25	1.0 (4)
N1—C2—C3—C4	−2.3 (4)	P1—C21—C26—C25	−177.5 (2)
C1—C2—C3—C4	175.1 (3)	C33—P1—C27—C32	7.0 (3)
C2—C3—C4—C5	0.3 (4)	C39—P1—C27—C32	−111.0 (2)
C3—C4—C5—C6	1.8 (4)	C21—P1—C27—C32	130.6 (2)
C2—N1—C6—C5	0.2 (4)	C33—P1—C27—C28	−175.9 (2)
Fe1—N1—C6—C5	−179.5 (2)	C39—P1—C27—C28	66.1 (2)
C4—C5—C6—N1	−2.2 (4)	C21—P1—C27—C28	−52.3 (2)
C11—N2—C7—C8	3.6 (3)	C32—C27—C28—C29	2.1 (4)
Fe1—N2—C7—C8	−169.12 (19)	P1—C27—C28—C29	−175.1 (2)
C11—N2—C7—C1	179.8 (2)	C27—C28—C29—C30	−1.6 (4)
Fe1—N2—C7—C1	7.0 (3)	C28—C29—C30—C31	0.4 (4)
C17—C1—C7—N2	175.4 (2)	C29—C30—C31—C32	0.4 (5)
C2—C1—C7—N2	52.7 (3)	C30—C31—C32—C27	0.1 (4)
C12—C1—C7—N2	−64.4 (3)	C28—C27—C32—C31	−1.3 (4)
C17—C1—C7—C8	−8.6 (3)	P1—C27—C32—C31	175.7 (2)
C2—C1—C7—C8	−131.2 (2)	C27—P1—C33—C34	120.0 (2)
C12—C1—C7—C8	111.7 (3)	C39—P1—C33—C34	−119.8 (2)
N2—C7—C8—C9	−1.3 (4)	C21—P1—C33—C34	−1.4 (3)
C1—C7—C8—C9	−177.2 (2)	C27—P1—C33—C38	−62.6 (2)
C7—C8—C9—C10	−1.2 (4)	C39—P1—C33—C38	57.5 (2)
C8—C9—C10—C11	1.2 (4)	C21—P1—C33—C38	176.0 (2)
C7—N2—C11—C10	−3.7 (4)	C38—C33—C34—C35	0.1 (4)
Fe1—N2—C11—C10	169.0 (2)	P1—C33—C34—C35	177.35 (19)
C9—C10—C11—N2	1.3 (4)	C33—C34—C35—C36	0.1 (4)
C16—N3—C12—C13	3.0 (4)	C34—C35—C36—C37	0.7 (4)
Fe1—N3—C12—C13	−176.42 (19)	C35—C36—C37—C38	−1.6 (4)
C16—N3—C12—C1	−175.4 (2)	C36—C37—C38—C33	1.8 (4)
Fe1—N3—C12—C1	5.2 (3)	C34—C33—C38—C37	−1.0 (4)
C17—C1—C12—N3	176.8 (2)	P1—C33—C38—C37	−178.4 (2)
C2—C1—C12—N3	−61.6 (3)	C33—P1—C39—C40	−143.5 (2)
C7—C1—C12—N3	56.8 (3)	C27—P1—C39—C40	−22.1 (2)
C17—C1—C12—C13	−1.5 (3)	C21—P1—C39—C40	95.9 (2)
C2—C1—C12—C13	120.1 (3)	C33—P1—C39—C44	41.3 (2)
C7—C1—C12—C13	−121.6 (3)	C27—P1—C39—C44	162.6 (2)
N3—C12—C13—C14	−3.1 (4)	C21—P1—C39—C44	−79.3 (2)
C1—C12—C13—C14	175.1 (2)	C44—C39—C40—C41	1.5 (4)
C12—C13—C14—C15	0.9 (4)	P1—C39—C40—C41	−173.7 (2)
C13—C14—C15—C16	1.3 (4)	C39—C40—C41—C42	−0.4 (4)
C12—N3—C16—C15	−0.7 (4)	C40—C41—C42—C43	−0.7 (4)
Fe1—N3—C16—C15	178.7 (2)	C41—C42—C43—C44	0.7 (4)
C14—C15—C16—N3	−1.4 (4)	C42—C43—C44—C39	0.5 (4)
C33—P1—C21—C26	−88.0 (2)	C40—C39—C44—C43	−1.6 (4)
C27—P1—C21—C26	148.4 (2)	P1—C39—C44—C43	173.8 (2)
C39—P1—C21—C26	29.1 (2)

(I296K) Tetraphenylphosphonium tris(thiocyanato-κN)[1,1,1-tris(pyridin-2-yl)ethane-κ³N,N',N'']ferrate(II)

Crystal data

(C24H20P)[Fe(NCS)3(C17H15N3)]	F(000) = 1720.00
Mr = 830.78	Dx = 1.323 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 9.069 (2) Å	Cell parameters from 10253 reflections
b = 15.984 (3) Å	θ = 2.3–25.7°
c = 28.820 (6) Å	µ = 0.59 mm^−1
β = 93.316 (18)°	T = 296 K
V = 4170.7 (16) Å^3	Block, red
Z = 4	0.45 × 0.35 × 0.30 mm

Data collection

Rigaku R-AXIS RAPID diffractometer	3173 reflections with F^2 > 2.0σ(F^2)
Detector resolution: 10.000 pixels mm^-1	Rint = 0.068
ω scans	θmax = 25.7°, θmin = 2.6°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −11→10
Tmin = 0.313, Tmax = 0.838	k = −19→18
21505 measured reflections	l = −35→35
7829 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.051	H-atom parameters constrained
S = 0.63	w = 1/[σ^2(Fo^2)]
7829 reflections	(Δ/σ)max = 0.001
496 parameters	Δρmax = 0.27 e Å^−3
0 restraints	Δρmin = −0.21 e Å^−3
Primary atom site location: structure-invariant direct methods

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	1.02003 (4)	0.23643 (2)	0.40158 (2)	0.04793 (12)
S1	1.37377 (9)	0.34500 (5)	0.51600 (3)	0.0833 (3)
S2	1.34031 (9)	0.00341 (5)	0.37799 (3)	0.0752 (3)
S3	1.25211 (10)	0.41611 (5)	0.29399 (3)	0.0922 (3)
P1	0.97168 (7)	0.23805 (4)	0.15225 (2)	0.04277 (18)
N1	0.8732 (2)	0.33542 (12)	0.40325 (6)	0.0395 (5)
N2	0.8706 (2)	0.18808 (11)	0.35068 (6)	0.0367 (5)
N3	0.8786 (2)	0.17910 (12)	0.44666 (6)	0.0443 (6)
N4	1.1490 (3)	0.28407 (14)	0.45500 (8)	0.0702 (8)
N5	1.1475 (3)	0.13214 (15)	0.39822 (8)	0.0661 (7)
N6	1.1318 (3)	0.29976 (14)	0.35232 (8)	0.0645 (7)
C1	0.6684 (2)	0.23396 (15)	0.39835 (7)	0.0368 (6)
C2	0.7262 (3)	0.32479 (15)	0.39998 (7)	0.0405 (7)
C3	0.6323 (3)	0.39274 (18)	0.39938 (9)	0.0688 (9)
H3	0.5307	0.3849	0.3957	0.083*
C4	0.6900 (4)	0.47252 (19)	0.40431 (10)	0.0801 (10)
H4	0.6274	0.5186	0.4043	0.096*
C5	0.8396 (4)	0.48342 (18)	0.40922 (9)	0.0646 (8)
H5	0.8805	0.5364	0.4135	0.078*
C6	0.9276 (3)	0.41367 (18)	0.40768 (7)	0.0541 (7)
H6	1.0296	0.4208	0.4098	0.065*
C7	0.7244 (3)	0.18679 (14)	0.35604 (8)	0.0354 (6)
C8	0.6313 (3)	0.14150 (15)	0.32623 (8)	0.0526 (7)
H8	0.5303	0.1412	0.3303	0.063*
C9	0.6869 (4)	0.09650 (17)	0.29030 (9)	0.0682 (9)
H9	0.6246	0.0645	0.2706	0.082*
C10	0.8363 (3)	0.09984 (17)	0.28409 (9)	0.0607 (8)
H10	0.8768	0.0714	0.2597	0.073*
C11	0.9239 (3)	0.14638 (15)	0.31489 (8)	0.0488 (7)
H11	1.0248	0.1491	0.3107	0.059*
C12	0.7305 (3)	0.18721 (14)	0.44197 (8)	0.0409 (7)
C13	0.6402 (3)	0.15355 (17)	0.47420 (10)	0.0685 (9)
H13	0.5386	0.1615	0.4711	0.082*
C14	0.7018 (5)	0.1086 (2)	0.51057 (11)	0.0915 (12)
H14	0.6418	0.0857	0.5324	0.110*
C15	0.8519 (5)	0.09693 (19)	0.51517 (11)	0.0837 (11)
H15	0.8949	0.0651	0.5394	0.100*
C16	0.9367 (3)	0.13410 (16)	0.48262 (10)	0.0617 (8)
H16	1.0387	0.1277	0.4857	0.074*
C17	0.4990 (2)	0.23388 (15)	0.39598 (8)	0.0598 (7)
H17A	0.4625	0.2632	0.3686	0.072*
H17B	0.4637	0.1773	0.3948	0.072*
H17C	0.4648	0.2611	0.4230	0.072*
C18	1.2405 (3)	0.30957 (16)	0.48085 (10)	0.0573 (8)
C19	1.2270 (3)	0.07833 (18)	0.39016 (9)	0.0526 (8)
C20	1.1810 (3)	0.34828 (18)	0.32792 (9)	0.0538 (8)
C21	0.8316 (3)	0.28044 (14)	0.18661 (9)	0.0468 (7)
C22	0.6902 (3)	0.29488 (17)	0.16658 (10)	0.0717 (9)
H22	0.6680	0.2837	0.1353	0.086*
C23	0.5834 (4)	0.3264 (2)	0.19452 (14)	0.0965 (12)
H23	0.4890	0.3362	0.1813	0.116*
C24	0.6115 (5)	0.3435 (2)	0.24026 (15)	0.0948 (13)
H24	0.5374	0.3642	0.2581	0.114*
C25	0.7503 (4)	0.32976 (18)	0.25975 (11)	0.0776 (10)
H25	0.7707	0.3409	0.2911	0.093*
C26	0.8611 (3)	0.29940 (14)	0.23314 (10)	0.0607 (8)
H26	0.9558	0.2917	0.2466	0.073*
C27	0.8846 (3)	0.17316 (15)	0.10842 (9)	0.0440 (7)
C28	0.7878 (3)	0.11047 (17)	0.12126 (10)	0.0622 (8)
H28	0.7646	0.1052	0.1521	0.075*
C29	0.7268 (3)	0.05652 (18)	0.08830 (13)	0.0756 (10)
H29	0.6651	0.0137	0.0973	0.091*
C30	0.7557 (4)	0.0651 (2)	0.04246 (12)	0.0858 (11)
H30	0.7126	0.0291	0.0202	0.103*
C31	0.8495 (4)	0.1276 (2)	0.02968 (10)	0.0855 (11)
H31	0.8693	0.1338	−0.0014	0.103*
C32	0.9142 (3)	0.18110 (17)	0.06228 (9)	0.0587 (8)
H32	0.9781	0.2227	0.0531	0.070*
C33	1.0789 (3)	0.31874 (16)	0.12732 (8)	0.0422 (7)
C34	1.0426 (3)	0.40189 (17)	0.13166 (8)	0.0517 (7)
H34	0.9599	0.4170	0.1474	0.062*
C35	1.1287 (3)	0.46305 (17)	0.11272 (9)	0.0630 (8)
H35	1.1042	0.5192	0.1158	0.076*
C36	1.2519 (4)	0.4405 (2)	0.08916 (9)	0.0705 (9)
H36	1.3105	0.4816	0.0767	0.085*
C37	1.2874 (3)	0.3576 (2)	0.08422 (9)	0.0747 (9)
H37	1.3688	0.3424	0.0679	0.090*
C38	1.2016 (3)	0.29646 (17)	0.10361 (9)	0.0642 (8)
H38	1.2265	0.2403	0.1007	0.077*
C39	1.0975 (3)	0.17772 (16)	0.18907 (8)	0.0417 (7)
C40	1.0840 (3)	0.09190 (17)	0.19362 (8)	0.0544 (7)
H40	1.0132	0.0630	0.1753	0.065*
C41	1.1755 (4)	0.04940 (18)	0.22533 (11)	0.0741 (9)
H41	1.1667	−0.0083	0.2282	0.089*
C42	1.2802 (3)	0.0918 (2)	0.25276 (10)	0.0807 (10)
H42	1.3414	0.0629	0.2742	0.097*
C43	1.2937 (3)	0.1765 (2)	0.24828 (10)	0.0797 (10)
H43	1.3642	0.2052	0.2668	0.096*
C44	1.2045 (3)	0.21929 (18)	0.21682 (9)	0.0630 (8)
H44	1.2153	0.2769	0.2139	0.076*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0444 (2)	0.0464 (3)	0.0538 (2)	−0.0058 (2)	0.00950 (19)	−0.0023 (2)
S1	0.0868 (7)	0.0824 (6)	0.0795 (6)	−0.0148 (6)	−0.0053 (5)	−0.0166 (5)
S2	0.0762 (6)	0.0622 (6)	0.0896 (6)	0.0103 (5)	0.0250 (5)	0.0186 (4)
S3	0.1172 (8)	0.0684 (6)	0.0963 (7)	0.0014 (6)	0.0508 (6)	0.0148 (5)
P1	0.0441 (5)	0.0419 (4)	0.0424 (4)	0.0011 (4)	0.0037 (4)	0.0040 (3)
N1	0.0381 (15)	0.0356 (14)	0.0447 (13)	−0.0064 (12)	0.0032 (11)	0.0007 (10)
N2	0.0375 (14)	0.0397 (13)	0.0338 (13)	−0.0011 (12)	0.0088 (11)	−0.0034 (9)
N3	0.0505 (16)	0.0426 (14)	0.0391 (14)	0.0034 (12)	−0.0026 (12)	0.0010 (10)
N4	0.0560 (17)	0.0636 (18)	0.092 (2)	−0.0026 (15)	0.0129 (15)	−0.0100 (14)
N5	0.0478 (18)	0.069 (2)	0.0820 (19)	−0.0083 (15)	0.0063 (14)	−0.0087 (14)
N6	0.0616 (18)	0.0701 (19)	0.0628 (18)	0.0018 (15)	0.0112 (14)	0.0021 (12)
C1	0.0283 (15)	0.0400 (16)	0.0428 (15)	−0.0059 (14)	0.0069 (12)	−0.0042 (13)
C2	0.0397 (19)	0.0412 (18)	0.0410 (16)	−0.0004 (16)	0.0053 (14)	−0.0024 (12)
C3	0.049 (2)	0.052 (2)	0.105 (3)	0.0040 (19)	0.0035 (17)	−0.0113 (17)
C4	0.079 (3)	0.041 (2)	0.120 (3)	0.020 (2)	0.009 (2)	−0.0040 (17)
C5	0.074 (3)	0.039 (2)	0.082 (2)	−0.005 (2)	0.0134 (19)	−0.0040 (15)
C6	0.055 (2)	0.050 (2)	0.0566 (19)	−0.0088 (19)	0.0055 (15)	−0.0024 (15)
C7	0.0316 (17)	0.0390 (16)	0.0358 (16)	−0.0006 (14)	0.0028 (13)	0.0014 (12)
C8	0.0399 (18)	0.0656 (19)	0.0523 (18)	−0.0048 (16)	0.0031 (15)	−0.0126 (15)
C9	0.073 (2)	0.080 (2)	0.051 (2)	−0.018 (2)	−0.0042 (18)	−0.0170 (16)
C10	0.066 (2)	0.068 (2)	0.0491 (19)	−0.005 (2)	0.0149 (17)	−0.0130 (15)
C11	0.0466 (18)	0.0563 (18)	0.0446 (17)	−0.0046 (16)	0.0122 (15)	−0.0032 (14)
C12	0.047 (2)	0.0371 (16)	0.0402 (17)	−0.0074 (15)	0.0155 (15)	−0.0059 (12)
C13	0.076 (2)	0.075 (2)	0.057 (2)	−0.011 (2)	0.0255 (19)	0.0108 (16)
C14	0.135 (4)	0.081 (3)	0.062 (3)	−0.016 (3)	0.039 (3)	0.0144 (19)
C15	0.144 (4)	0.060 (2)	0.047 (2)	0.006 (3)	−0.005 (3)	0.0090 (16)
C16	0.079 (2)	0.0519 (19)	0.053 (2)	0.0051 (18)	−0.0103 (19)	−0.0024 (15)
C17	0.0430 (18)	0.0650 (19)	0.0722 (19)	−0.0011 (17)	0.0105 (14)	−0.0151 (15)
C18	0.064 (2)	0.0421 (19)	0.069 (2)	0.0008 (17)	0.0276 (18)	−0.0044 (15)
C19	0.042 (2)	0.061 (2)	0.0546 (19)	−0.0180 (17)	0.0012 (15)	0.0051 (16)
C20	0.044 (2)	0.064 (2)	0.055 (2)	0.0109 (18)	0.0080 (15)	−0.0044 (15)
C21	0.052 (2)	0.0451 (17)	0.0447 (18)	−0.0035 (16)	0.0121 (15)	0.0055 (14)
C22	0.049 (2)	0.089 (3)	0.079 (2)	0.0033 (19)	0.018 (2)	0.0034 (17)
C23	0.052 (2)	0.102 (3)	0.139 (4)	0.009 (2)	0.034 (3)	0.009 (3)
C24	0.106 (4)	0.060 (2)	0.127 (4)	0.004 (3)	0.075 (3)	0.004 (2)
C25	0.115 (3)	0.050 (2)	0.072 (2)	0.003 (2)	0.043 (3)	0.0026 (16)
C26	0.075 (2)	0.0448 (18)	0.064 (2)	0.0051 (17)	0.0221 (19)	0.0042 (15)
C27	0.0429 (18)	0.0448 (17)	0.0439 (18)	0.0007 (15)	−0.0007 (14)	0.0036 (13)
C28	0.059 (2)	0.063 (2)	0.065 (2)	−0.0140 (18)	0.0038 (17)	−0.0013 (16)
C29	0.061 (2)	0.067 (2)	0.096 (3)	−0.0254 (18)	−0.017 (2)	0.000 (2)
C30	0.098 (3)	0.071 (3)	0.084 (3)	−0.001 (2)	−0.037 (2)	−0.019 (2)
C31	0.124 (3)	0.077 (3)	0.054 (2)	0.001 (2)	−0.015 (2)	−0.0017 (19)
C32	0.073 (2)	0.0535 (19)	0.0484 (19)	−0.0059 (17)	−0.0041 (17)	0.0049 (15)
C33	0.0425 (19)	0.0394 (18)	0.0450 (17)	−0.0004 (15)	0.0047 (14)	0.0066 (12)
C34	0.053 (2)	0.049 (2)	0.0537 (19)	−0.0020 (18)	0.0074 (15)	0.0011 (14)
C35	0.070 (2)	0.048 (2)	0.071 (2)	−0.0076 (19)	0.0035 (18)	0.0036 (15)
C36	0.073 (3)	0.059 (2)	0.079 (2)	−0.022 (2)	0.0085 (19)	0.0171 (17)
C37	0.059 (2)	0.070 (2)	0.099 (3)	−0.005 (2)	0.0364 (18)	0.0124 (19)
C38	0.060 (2)	0.052 (2)	0.082 (2)	0.0067 (18)	0.0215 (18)	0.0076 (15)
C39	0.0413 (18)	0.0434 (18)	0.0403 (16)	0.0009 (15)	0.0007 (14)	−0.0006 (13)
C40	0.059 (2)	0.047 (2)	0.0568 (19)	0.0070 (17)	−0.0010 (16)	0.0003 (15)
C41	0.079 (2)	0.055 (2)	0.088 (3)	0.018 (2)	0.005 (2)	0.0176 (19)
C42	0.065 (3)	0.097 (3)	0.078 (3)	0.011 (2)	−0.015 (2)	0.029 (2)
C43	0.066 (2)	0.088 (3)	0.083 (3)	−0.009 (2)	−0.015 (2)	0.018 (2)
C44	0.0575 (19)	0.062 (2)	0.068 (2)	−0.0010 (19)	−0.0098 (17)	0.0160 (17)

Geometric parameters (Å, º)

Fe1—N4	2.027 (2)	C16—H16	0.9300
Fe1—N5	2.034 (2)	C17—H17A	0.9600
Fe1—N6	2.058 (2)	C17—H17B	0.9600
Fe1—N1	2.0701 (19)	C17—H17C	0.9600
Fe1—N2	2.0873 (19)	C21—C26	1.386 (3)
Fe1—N3	2.089 (2)	C21—C22	1.394 (3)
S1—C18	1.633 (3)	C22—C23	1.389 (4)
S2—C19	1.629 (3)	C22—H22	0.9300
S3—C20	1.619 (3)	C23—C24	1.356 (4)
P1—C27	1.783 (2)	C23—H23	0.9300
P1—C21	1.789 (3)	C24—C25	1.366 (4)
P1—C33	1.790 (2)	C24—H24	0.9300
P1—C39	1.794 (2)	C25—C26	1.387 (3)
N1—C2	1.342 (3)	C25—H25	0.9300
N1—C6	1.348 (3)	C26—H26	0.9300
N2—C11	1.342 (2)	C27—C32	1.378 (3)
N2—C7	1.343 (3)	C27—C28	1.396 (3)
N3—C16	1.344 (3)	C28—C29	1.375 (3)
N3—C12	1.348 (3)	C28—H28	0.9300
N4—C18	1.157 (3)	C29—C30	1.369 (3)
N5—C19	1.155 (3)	C29—H29	0.9300
N6—C20	1.154 (3)	C30—C31	1.376 (4)
C1—C17	1.534 (3)	C30—H30	0.9300
C1—C12	1.541 (3)	C31—C32	1.377 (3)
C1—C2	1.543 (3)	C31—H31	0.9300
C1—C7	1.544 (3)	C32—H32	0.9300
C2—C3	1.380 (3)	C33—C34	1.377 (3)
C3—C4	1.383 (3)	C33—C38	1.386 (3)
C3—H3	0.9300	C34—C35	1.383 (3)
C4—C5	1.367 (3)	C34—H34	0.9300
C4—H4	0.9300	C35—C36	1.388 (3)
C5—C6	1.373 (3)	C35—H35	0.9300
C5—H5	0.9300	C36—C37	1.374 (3)
C6—H6	0.9300	C36—H36	0.9300
C7—C8	1.375 (3)	C37—C38	1.386 (3)
C8—C9	1.380 (3)	C37—H37	0.9300
C8—H8	0.9300	C38—H38	0.9300
C9—C10	1.378 (3)	C39—C40	1.384 (3)
C9—H9	0.9300	C39—C44	1.390 (3)
C10—C11	1.375 (3)	C40—C41	1.378 (3)
C10—H10	0.9300	C40—H40	0.9300
C11—H11	0.9300	C41—C42	1.378 (4)
C12—C13	1.382 (3)	C41—H41	0.9300
C13—C14	1.363 (4)	C42—C43	1.366 (4)
C13—H13	0.9300	C42—H42	0.9300
C14—C15	1.372 (4)	C43—C44	1.364 (3)
C14—H14	0.9300	C43—H43	0.9300
C15—C16	1.382 (4)	C44—H44	0.9300
C15—H15	0.9300
N4—Fe1—N5	92.26 (9)	C15—C16—H16	118.5
N4—Fe1—N6	93.07 (10)	C1—C17—H17A	109.5
N5—Fe1—N6	93.81 (9)	C1—C17—H17B	109.5
N4—Fe1—N1	92.23 (8)	H17A—C17—H17B	109.5
N5—Fe1—N1	174.55 (9)	C1—C17—H17C	109.5
N6—Fe1—N1	89.04 (9)	H17A—C17—H17C	109.5
N4—Fe1—N2	174.58 (9)	H17B—C17—H17C	109.5
N5—Fe1—N2	90.61 (8)	N4—C18—S1	178.0 (3)
N6—Fe1—N2	91.32 (9)	N5—C19—S2	178.9 (3)
N1—Fe1—N2	84.67 (8)	N6—C20—S3	179.2 (3)
N4—Fe1—N3	92.32 (9)	C26—C21—C22	119.1 (3)
N5—Fe1—N3	92.34 (9)	C26—C21—P1	121.0 (2)
N6—Fe1—N3	171.65 (9)	C22—C21—P1	119.9 (2)
N1—Fe1—N3	84.38 (8)	C23—C22—C21	118.4 (3)
N2—Fe1—N3	82.97 (8)	C23—C22—H22	120.8
C27—P1—C21	108.23 (12)	C21—C22—H22	120.8
C27—P1—C33	111.31 (12)	C24—C23—C22	122.6 (4)
C21—P1—C33	111.65 (12)	C24—C23—H23	118.7
C27—P1—C39	110.29 (12)	C22—C23—H23	118.7
C21—P1—C39	108.90 (11)	C23—C24—C25	118.9 (4)
C33—P1—C39	106.44 (12)	C23—C24—H24	120.5
C2—N1—C6	118.7 (2)	C25—C24—H24	120.5
C2—N1—Fe1	122.63 (18)	C24—C25—C26	120.6 (3)
C6—N1—Fe1	118.63 (19)	C24—C25—H25	119.7
C11—N2—C7	118.9 (2)	C26—C25—H25	119.7
C11—N2—Fe1	118.41 (18)	C21—C26—C25	120.4 (3)
C7—N2—Fe1	121.98 (16)	C21—C26—H26	119.8
C16—N3—C12	118.2 (2)	C25—C26—H26	119.8
C16—N3—Fe1	119.14 (19)	C32—C27—C28	118.9 (2)
C12—N3—Fe1	122.62 (17)	C32—C27—P1	121.8 (2)
C18—N4—Fe1	169.2 (3)	C28—C27—P1	119.3 (2)
C19—N5—Fe1	169.5 (3)	C29—C28—C27	120.1 (3)
C20—N6—Fe1	167.0 (2)	C29—C28—H28	120.0
C17—C1—C12	110.7 (2)	C27—C28—H28	120.0
C17—C1—C2	109.8 (2)	C30—C29—C28	120.8 (3)
C12—C1—C2	108.90 (18)	C30—C29—H29	119.6
C17—C1—C7	109.8 (2)	C28—C29—H29	119.6
C12—C1—C7	106.61 (19)	C29—C30—C31	119.2 (3)
C2—C1—C7	110.90 (18)	C29—C30—H30	120.4
N1—C2—C3	120.7 (2)	C31—C30—H30	120.4
N1—C2—C1	117.1 (2)	C30—C31—C32	120.9 (3)
C3—C2—C1	122.1 (2)	C30—C31—H31	119.5
C2—C3—C4	119.7 (3)	C32—C31—H31	119.5
C2—C3—H3	120.2	C31—C32—C27	120.1 (3)
C4—C3—H3	120.2	C31—C32—H32	119.9
C5—C4—C3	119.7 (3)	C27—C32—H32	119.9
C5—C4—H4	120.1	C34—C33—C38	119.7 (2)
C3—C4—H4	120.1	C34—C33—P1	121.4 (2)
C4—C5—C6	117.9 (3)	C38—C33—P1	118.9 (2)
C4—C5—H5	121.0	C33—C34—C35	120.2 (3)
C6—C5—H5	121.0	C33—C34—H34	119.9
N1—C6—C5	123.1 (3)	C35—C34—H34	119.9
N1—C6—H6	118.5	C34—C35—C36	119.9 (3)
C5—C6—H6	118.5	C34—C35—H35	120.1
N2—C7—C8	120.7 (2)	C36—C35—H35	120.1
N2—C7—C1	117.1 (2)	C37—C36—C35	120.1 (3)
C8—C7—C1	122.1 (2)	C37—C36—H36	119.9
C7—C8—C9	120.4 (3)	C35—C36—H36	119.9
C7—C8—H8	119.8	C36—C37—C38	119.8 (3)
C9—C8—H8	119.8	C36—C37—H37	120.1
C10—C9—C8	118.8 (3)	C38—C37—H37	120.1
C10—C9—H9	120.6	C37—C38—C33	120.2 (3)
C8—C9—H9	120.6	C37—C38—H38	119.9
C11—C10—C9	118.2 (3)	C33—C38—H38	119.9
C11—C10—H10	120.9	C40—C39—C44	118.8 (3)
C9—C10—H10	120.9	C40—C39—P1	122.2 (2)
N2—C11—C10	123.0 (2)	C44—C39—P1	118.8 (2)
N2—C11—H11	118.5	C41—C40—C39	119.9 (3)
C10—C11—H11	118.5	C41—C40—H40	120.1
N3—C12—C13	121.4 (3)	C39—C40—H40	120.1
N3—C12—C1	116.3 (2)	C40—C41—C42	120.4 (3)
C13—C12—C1	122.3 (3)	C40—C41—H41	119.8
C14—C13—C12	119.3 (3)	C42—C41—H41	119.8
C14—C13—H13	120.3	C43—C42—C41	119.7 (3)
C12—C13—H13	120.3	C43—C42—H42	120.1
C13—C14—C15	120.4 (3)	C41—C42—H42	120.1
C13—C14—H14	119.8	C44—C43—C42	120.5 (3)
C15—C14—H14	119.8	C44—C43—H43	119.8
C14—C15—C16	117.7 (3)	C42—C43—H43	119.8
C14—C15—H15	121.2	C43—C44—C39	120.7 (3)
C16—C15—H15	121.2	C43—C44—H44	119.7
N3—C16—C15	123.0 (3)	C39—C44—H44	119.7
N3—C16—H16	118.5
C6—N1—C2—C3	2.4 (3)	C27—P1—C21—C22	−30.1 (2)
Fe1—N1—C2—C3	−177.40 (17)	C33—P1—C21—C22	92.7 (2)
C6—N1—C2—C1	−175.90 (18)	C39—P1—C21—C22	−150.0 (2)
Fe1—N1—C2—C1	4.3 (3)	C26—C21—C22—C23	−1.2 (4)
C17—C1—C2—N1	178.5 (2)	P1—C21—C22—C23	178.8 (2)
C12—C1—C2—N1	57.0 (3)	C21—C22—C23—C24	0.0 (5)
C7—C1—C2—N1	−60.0 (3)	C22—C23—C24—C25	0.4 (5)
C17—C1—C2—C3	0.1 (3)	C23—C24—C25—C26	0.4 (5)
C12—C1—C2—C3	−121.3 (2)	C22—C21—C26—C25	2.1 (4)
C7—C1—C2—C3	121.7 (2)	P1—C21—C26—C25	−177.97 (19)
N1—C2—C3—C4	−2.9 (4)	C24—C25—C26—C21	−1.7 (4)
C1—C2—C3—C4	175.3 (2)	C21—P1—C27—C32	130.0 (2)
C2—C3—C4—C5	0.7 (4)	C33—P1—C27—C32	7.0 (2)
C3—C4—C5—C6	1.9 (4)	C39—P1—C27—C32	−110.9 (2)
C2—N1—C6—C5	0.3 (3)	C21—P1—C27—C28	−52.4 (2)
Fe1—N1—C6—C5	−179.89 (18)	C33—P1—C27—C28	−175.4 (2)
C4—C5—C6—N1	−2.4 (4)	C39—P1—C27—C28	66.6 (2)
C11—N2—C7—C8	1.9 (3)	C32—C27—C28—C29	1.7 (4)
Fe1—N2—C7—C8	−168.19 (17)	P1—C27—C28—C29	−176.0 (2)
C11—N2—C7—C1	178.6 (2)	C27—C28—C29—C30	−2.2 (4)
Fe1—N2—C7—C1	8.5 (3)	C28—C29—C30—C31	1.3 (5)
C17—C1—C7—N2	173.9 (2)	C29—C30—C31—C32	0.2 (5)
C12—C1—C7—N2	−66.1 (3)	C30—C31—C32—C27	−0.6 (4)
C2—C1—C7—N2	52.3 (3)	C28—C27—C32—C31	−0.3 (4)
C17—C1—C7—C8	−9.5 (3)	P1—C27—C32—C31	177.3 (2)
C12—C1—C7—C8	110.5 (2)	C27—P1—C33—C34	115.2 (2)
C2—C1—C7—C8	−131.0 (2)	C21—P1—C33—C34	−5.9 (2)
N2—C7—C8—C9	0.1 (4)	C39—P1—C33—C34	−124.6 (2)
C1—C7—C8—C9	−176.5 (2)	C27—P1—C33—C38	−65.5 (2)
C7—C8—C9—C10	−1.9 (4)	C21—P1—C33—C38	173.47 (19)
C8—C9—C10—C11	1.7 (4)	C39—P1—C33—C38	54.8 (2)
C7—N2—C11—C10	−2.2 (4)	C38—C33—C34—C35	−0.5 (4)
Fe1—N2—C11—C10	168.3 (2)	P1—C33—C34—C35	178.92 (19)
C9—C10—C11—N2	0.4 (4)	C33—C34—C35—C36	0.2 (4)
C16—N3—C12—C13	2.8 (4)	C34—C35—C36—C37	0.7 (4)
Fe1—N3—C12—C13	−175.31 (17)	C35—C36—C37—C38	−1.3 (4)
C16—N3—C12—C1	−175.8 (2)	C36—C37—C38—C33	1.0 (4)
Fe1—N3—C12—C1	6.1 (3)	C34—C33—C38—C37	−0.1 (4)
C17—C1—C12—N3	176.6 (2)	P1—C33—C38—C37	−179.5 (2)
C2—C1—C12—N3	−62.6 (3)	C27—P1—C39—C40	−22.8 (2)
C7—C1—C12—N3	57.2 (3)	C21—P1—C39—C40	95.8 (2)
C17—C1—C12—C13	−2.0 (3)	C33—P1—C39—C40	−143.7 (2)
C2—C1—C12—C13	118.8 (2)	C27—P1—C39—C44	162.6 (2)
C7—C1—C12—C13	−121.4 (2)	C21—P1—C39—C44	−78.8 (2)
N3—C12—C13—C14	−2.5 (4)	C33—P1—C39—C44	41.7 (2)
C1—C12—C13—C14	176.1 (3)	C44—C39—C40—C41	0.1 (4)
C12—C13—C14—C15	0.1 (5)	P1—C39—C40—C41	−174.4 (2)
C13—C14—C15—C16	1.7 (5)	C39—C40—C41—C42	0.3 (4)
C12—N3—C16—C15	−0.9 (4)	C40—C41—C42—C43	−0.4 (5)
Fe1—N3—C16—C15	177.3 (2)	C41—C42—C43—C44	−0.1 (5)
C14—C15—C16—N3	−1.4 (5)	C42—C43—C44—C39	0.6 (5)
C27—P1—C21—C26	149.91 (19)	C40—C39—C44—C43	−0.6 (4)
C33—P1—C21—C26	−87.2 (2)	P1—C39—C44—C43	174.2 (2)
C39—P1—C21—C26	30.0 (2)